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Potassium Carbonate → HCID 86601408、化合物

HRID 854198
ノート
印刷プレビュー

反応式

HRID 854198 の反応式
C([O:4][CH:5]1[CH:6]([CH3:53])[CH2:7][CH2:8][CH:9]([O:47][CH:48]([O:50][CH2:51][CH3:52])[CH3:49])[CH2:10][C:11]([O:13][CH:14](/[C:19](/[CH3:46])=[CH:20]/[CH:21]=[CH:22]/[C:23]([O:40][CH:41]([O:43][CH2:44][CH3:45])[CH3:42])([CH3:39])[CH2:24][CH:25]2[O:38][CH:26]2[CH:27]([CH3:37])[CH:28]([O:31][CH:32]([O:34][CH2:35][CH3:36])[CH3:33])[CH2:29][CH3:30])[CH:15]([CH3:18])[CH:16]=[CH:17]1)=[O:12])(=O)C.C(=O)([O-])[O-].[K+].[K+]>CO.C(OCC)(=O)C>[CH2:51]([O:50][CH:48]([O:47][CH:9]1[CH2:8][CH2:7][CH:6]([CH3:53])[CH:5]([OH:4])[CH:17]=[CH:16][CH:15]([CH3:18])[CH:14](/[C:19](/[CH3:46])=[CH:20]/[CH:21]=[CH:22]/[C:23]([O:40][CH:41]([O:43][CH2:44][CH3:45])[CH3:42])([CH3:39])[CH2:24][CH:25]2[O:38][CH:26]2[CH:27]([CH3:37])[CH:28]([O:31][CH:32]([O:34][CH2:35][CH3:36])[CH3:33])[CH2:29][CH3:30])[O:13][C:11](=[O:12])[CH2:10]1)[CH3:49])[CH3:52]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

HCID 11430Potassium CarbonateHCID 86601409HCID 86601409、化合物

生成物 1

HCID 86601408HCID 86601408、化合物収率 78.6%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 8857Ethyl Acetate溶媒

実験手順

(8E,12E,14E)-7-acetoxy-3,16,21-tris(1-ethoxyethoxy)-6,10,12,16,20-pentamethyl-18,19-epoxytricosa-8,12,14-trien-11-olide (186 mg) as the crude product was dissolved in methanol (2 mL). Potassium carbonate (75.0 mg, 543 μmol) was added to the reaction mixture, and the reaction mixture was stirred at room temperature for three hours. This reaction solution was diluted with ethyl acetate (50 mL), and the organic layer was washed with brine (10 mL) twice. The organic layer was dried over anhydrous sodium sulfate, filtered and concentrated. The resulting concentrate was purified by silica gel column chromatography (Merck Silica gel 60, 63 to 200 μm; hexane:ethyl acetate=3:1->2:1) to obtain the title compound (131 mg, 185 μmol, 78.6%, 2 steps) as a colorless oil.

後処理

  1. washthe organic layer was washed with brine (10 mL) twice
  2. dry with materialThe organic layer was dried over anhydrous sodium sulfate
  3. filtrationfiltered
  4. concentrationconcentrated
  5. concentrationThe resulting concentrate
  6. customwas purified by silica gel column chromatography (Merck Silica gel 60, 63 to 200 μm; hexane:ethyl acetate=3:1->2:1)

出典と根拠

ORDレコード
ord-0242ecc1733b4d3da783f3c5106c31b4
出典データセット
uspto-grants-2007_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07256178B2

反応ノート

読み込み中…

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